Synthesis and characterization of crown ether–containing N‐phosphorylated thioureas RC(S)NHP(O)(OiPr)2 (R = 1‐aza‐15‐crown‐5, 1‐aza‐12‐crown‐4) and their Co(II) and Ni(II) complexes

Reaction of piperazine with isothiocyanate (iPrO)2P(S)NCS leads to N-thiophosphorylated bis-thiourea (iPrO)2P(S)NHC(S)NC4H8NC(S)NHP(S)(OiPr)2 (H2L). Recrystallization of H2L from DMSO leads to the formation of the new ligand (iPrO)2P(S)NC4H8NP(S)(OiPr)2 (1). Reaction of doubly deprotonated L with Co(II) leads to the [Co2L2] complex. The thermal properties of [Co2L2] in an air atmosphere were studied by means of TGA with the observed final residue corresponding to [CoPS3]2. The crystal structure of [Co2L2] was elucidated by single crystal X-ray diffraction. Two metal cations are in a tetrahedral 1,5-S2S'2 environment formed by the C=S and P=S sulfur atoms. Investigation of the temperature dependence of the magnetic susceptibility is consistent with two effectively non-interacting Co(II) S = 3/2 ions.

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A novel amido–pyrophosphate Mn^IIchelate complex with the synthetic ligand O{P(O)[NHC(CH₃)₃]₂}₂(L): [Mn(L)₂{OC(H)N(CH₃)₂}₂]Cl₂·2H₂O

Tarahhomi

Pourayoubi

Fejfarová

et al. 2013

Acta Crystallogr C

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The title complex, trans-bis(dimethylformamide-κO)bis{N,N'-N'',N'''-tetra-tert-butyl[oxybis(phosphonic diamide-κO)]}manganese(II) dichloride dihydrate, [Mn(C16H40N4O3P2)2(C3H7NO)2]Cl2·2H2O, is the first example of a bis-chelate amido-pyrophosphate (pyrophosphoramide) complex containing an O[P(O)(NH)2]2 fragment. Its asymmetric unit contains half of the complex dication, one chloride anion and one water molecule. The Mn(II) atom, located on an inversion centre, is octahedrally coordinated, with a slight elongation towards the monodentate dimethylformamide ligand. Structural features of the title complex, such as the P=O bond lengths and the planarity of the chelate ring, are compared with those of previously reported complexes with six-membered chelates involving the fragments C(O)NHP(O), (X)NP(O) [X = C(O), C(S), S(O)2 and P(O)] and O[P(O)(N)2]2. This analysis shows that the six-membered chelate rings are less puckered in pyrophosphoramide complexes containing a P(O)OP(O) skeleton, such as the title compound. The extended structure of the title complex involves a linear aggregate mediated by N-H...O and N-H...Cl hydrogen bonds, in which the chloride anion is an acceptor in two additional O-H...Cl hydrogen bonds.

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Synthesis and characterization of crown ether–containing N‐phosphorylated thioureas RC(S)NHP(O)(OiPr)₂ (R = 1‐aza‐15‐crown‐5, 1‐aza‐12‐crown‐4) and their Co(II) and Ni(II) complexes

Abstract: The reaction of the lithium salts of N-phosphorylated thioureas RC(S)NHP(O)(OiPr) -aza-15-crown-5

Cited by 3 publications

References 29 publications

Synthesis and cation binding of acridono-18-crown-6 ether type ligands

Synthesis and cation binding of acridono-18-crown-6 ether type ligands

First structurally characterized self-assembly of bipodal N-thiophosphorylated bis-thiourea with CoII: magnetic properties and thermal decomposition

A novel amido–pyrophosphate Mn^IIchelate complex with the synthetic ligand O{P(O)[NHC(CH₃)₃]₂}₂(L): [Mn(L)₂{OC(H)N(CH₃)₂}₂]Cl₂·2H₂O

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Synthesis and characterization of crown ether–containing N‐phosphorylated thioureas RC(S)NHP(O)(OiPr)2 (R = 1‐aza‐15‐crown‐5, 1‐aza‐12‐crown‐4) and their Co(II) and Ni(II) complexes

Abstract: The reaction of the lithium salts of N-phosphorylated thioureas RC(S)NHP(O)(OiPr) -aza-15-crown-5

Cited by 3 publications

References 29 publications

Synthesis and cation binding of acridono-18-crown-6 ether type ligands

Synthesis and cation binding of acridono-18-crown-6 ether type ligands

First structurally characterized self-assembly of bipodal N-thiophosphorylated bis-thiourea with CoII: magnetic properties and thermal decomposition

A novel amido–pyrophosphate MnIIchelate complex with the synthetic ligand O{P(O)[NHC(CH3)3]2}2(L): [Mn(L)2{OC(H)N(CH3)2}2]Cl2·2H2O

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Synthesis and characterization of crown ether–containing N‐phosphorylated thioureas RC(S)NHP(O)(OiPr)₂ (R = 1‐aza‐15‐crown‐5, 1‐aza‐12‐crown‐4) and their Co(II) and Ni(II) complexes

A novel amido–pyrophosphate Mn^IIchelate complex with the synthetic ligand O{P(O)[NHC(CH₃)₃]₂}₂(L): [Mn(L)₂{OC(H)N(CH₃)₂}₂]Cl₂·2H₂O